P
US7045109B2ExpiredUtilityPatentIndex 50

Conversion of sodium bromide to anhydrous hydrobromic acid and sodium bisulfate

Assignee: PROCTER & GAMBLEPriority: Oct 7, 2002Filed: Nov 19, 2004Granted: May 16, 2006
Est. expiryOct 7, 2022(expired)· nominal 20-yr term from priority
Inventors:SCHAEFER JARED JOHNKENNEALLY COREY JAMESBOURGEOIS DANIEL MARTINBACK DEBORAH JEAN
C01D 5/02C01B 7/093
50
PatentIndex Score
1
Cited by
16
References
26
Claims

Abstract

Process for the conversion of sodium bromide to anhydrous hydrobromic acid and sodium bisulfate, said process with the following sequential steps: reaction of sodium bromide and sulfuric acid in a solution of water to produce hydrobromic acid and sodium bisulfate wherein the conversion of sodium bromide is greater than about 99%; adsorption of iron bromide onto a solid adsorbent; separation of hydrobromic acid and water from the sodium bisulfate; separation and drying of hydrobromic acid; and solidification of the sodium bisulfate into a flaked or granular form.

Claims

exact text as granted — not AI-modified
1. A process for the conversion of sodium bromide to anhydrous hydrobromic acid and sodium bisulfate, said process comprising the following sequential steps:
 a) reaction of sodium bromide and sulfuric acid in a solution of water to produce hydrobromic acid and sodium bisulfate wherein the conversion of sodium bromide is greater than about 99%; 
 b) separation of hydrobromic acid and water from the sodium bisulfate; and 
 c) separation of hydrobromic acid from water; followed by drying of hydrobromic acid. 
 
     
     
       2. A process according to  claim 1  wherein the process further includes the step of absorption of iron bromide onto a solid adsorbent, before the separation of hydrobromic acid and water from the sodium bisulfate. 
     
     
       3. A process according to  claim 2  wherein a chemical additive is included with the reaction of sodium bromide and sulfuric acid in a solution of water. 
     
     
       4. A process according to  claim 1  wherein the separation of hydrobromic acid and water from the sodium bisulfate takes place at a temperature less than about 270° C. 
     
     
       5. A process according to  claim 1  wherein the process further includes the step of solidifying the sodium bisulfate into a flaked, or granular form after the drying of hydrobromic acid. 
     
     
       6. A process according to  claim 1  wherein the reaction step (a) uses a reactor device selected from the group consisting of tanks, columns, pipes, and mixtures thereof. 
     
     
       7. A process according to  claim 5  wherein the reactor device is selected from the group consisting of columns, pipes, and mixtures thereof, and further comprises an internal blending device selected from the group consisting of orifice plates, segmented baffles, static mixers, and mixtures thereof. 
     
     
       8. A process according to  claim 1  wherein the reactor device is a pipe and wherein the blending is provided solely by a pump which operates in a turbulent flow regime. 
     
     
       9. A process according to  claim 5  wherein the temperature used for solidification is from about 180° C. to about 220° C. 
     
     
       10. A process according to  claim 6  wherein the molar ratio of sulfuric acid to sodium bromide is from about 0.95 to about 1.05 and the ratio of sodium bromide to water is less than about 0.9 parts by weight sodium bromide to 1 part water. 
     
     
       11. A process according to  claim 10  wherein the sulfuric acid is added slowly to the sodium bromide solution. 
     
     
       12. A process according to  claim 10  wherein the temperature for the reaction is from about 20° C. to about 180° C. at one atmosphere pressure. 
     
     
       13. A process according to  claim 6  wherein the separation of hydrobromic acid and water from the sodium bisulfate step (b) uses a separation device selected from the group consisting of evaporators, dryers, crystallizers, centrifuges, filters, and mixtures thereof. 
     
     
       14. A process according to  claim 13  wherein the separation device is selected from the group consisting of evaporators, dryers, and mixtures thereof, wherein the evaporators are selected from the group consisting of forced circulation, vertical and horizontal tube, jacketed kettles, agitated thin film devices, and mixtures thereof and wherein the dryers are selected from the group consisting of pan dryers, indirect rotary dryers, fluidized beds, spray dryers, drum dryers, and mixtures thereof. 
     
     
       15. A process according to  claim 14  wherein the separation device is a forced circulation evaporator. 
     
     
       16. A process according to  claim 13  wherein the exposure time to temperatures above 200° C. during the separation step (b) is less than 10 minutes. 
     
     
       17. A process according to  claim 14  wherein the separation device is an evaporator and the sodium bisulfate is in a molten state. 
     
     
       18. A process according to  claim 1  wherein the separation of hydrobromic acid from water step (c) uses an approach selected from the group consisting of multi-stage distillation, liquid extraction, membrane separation, and mixtures thereof. 
     
     
       19. A process according to  claim 18  wherein the step (c) approach is azeotropic distillation. 
     
     
       20. A process according to  claim 19  wherein the step (c) approach is pressure swing azeotropic distillation. 
     
     
       21. A process according to  claim 1  wherein the drying of hydrobromic acid step (d) results in a hydrobromic acid product having a moisture content of less than about 0.4%, by weight. 
     
     
       22. A process according to  claim 21  wherein the drying of hydrobromic acid step (d) uses a drying approach selected from the group consisting of distillation, stripping, solids adsorption, gas separation membranes, gas absorption, or mixtures thereof. 
     
     
       23. A process according to  claim 22  wherein the drying step (d) uses distillation. 
     
     
       24. A process for the conversion of sodium bromide to anhydrous hydrobromic acid and a sodium bisulfate coproduct, said process comprising the following sequential steps:
 a) reaction of sodium bromide and sulfuric acid in a solution of water to produce hydrobromic acid and sodium bisulfate wherein the conversion of sodium bromide is greater than about 99% by means of an adiabatic ioop reactor and wherein the molar ratio of sulfuric acid to sodium bromide is from about 0.95 to about 1.05 and the ratio of sodium bromide to water is less than about 0.9 parts by weight sodium bromide to 1 part water; 
 b) separation of hydrobromic acid and water from the sodium bisulfate by means of a forced circulation evaporator; 
 c) separation of hydrobromic acid from water by means of azeotropic distillation; and 
 d) drying of hydrobromic acid. 
 
     
     
       25. A process for the conversion of sodium bromide to anhydrous hydrobromic acid and a sodium bisulfate coproduct, said process comprising the following sequential steps:
 a) reaction of sodium bromide and sulfuric acid in a solution of water to produce hydrobromic acid and sodium bisulfate wherein a chemical additive is included with the reaction of sodium bromide and sulfuric acid in the solution of water; wherein the conversion of sodium bromide is greater than about 99%, by means of an adiabatic loop reactor and wherein the molar ratio of sulfuric acid to sodium bromide is from about 0.95 to about 1.05 and the ratio of sodium bromide to water is less than about 0.9 parts by weight sodium bromide to 1 part water; 
 b) absorption of iron bromide onto a solid adsorbent; 
 c) separation of hydrobromic acid and water from the sodium bisulfate by means of a forced circulation evaporator; 
 d) separation of hydrobromic acid from water by means of azeotropic distillation; 
 e) drying of hydrobromic acid; and 
 f) solidifying the sodium bisulfate into a form selected from the group consisting of flaked, granular, and mixtures thereof. 
 
     
     
       26. A process for the conversion of sodium bromide to anhydrous hydrobromic acid and a sodium bisulfate coproduct, said process comprising the following sequential steps:
 a) reaction of sodium bromide and sulfuric acid in a solution of water to produce hydrobromic acid and sodium bisulfate wherein a chemical additive is included with the reaction of sodium bromide and sulfuric acid in the solution of water; wherein the conversion of sodium bromide is greater than about 99%, by means of an adiabatic loop reactor and wherein the molar ratio of sulfuric acid to sodium bromide is from about 0.95 to about 1.05 and the ratio of sodium bromide to water is less than about 0.9 parts by weight sodium bromide to 1 part water; 
 b) separation of the hydrobromic acid and water from the sodium bisulfate by means of a forced circulation evaporator at a temperature less than about 270° C.; 
 c) separation of the hydrobromic acid from water by means of azeotropic distillation; 
 d) drying of the hydrobromic acid; and 
 e) solidifying the sodium bisulfate into a form selected from flaked, granular, and mixtures thereof.

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